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DOE OSTI2022

A High-Throughput MEMS-Based Differential Scanning Calorimeter for Direct Thermal Characterization of Antibodies

Calorimeters, which can be used for rapid thermal characterization of biomolecules, are getting intense attention in drug development. This paper presents a novel MEMS-based differential scanning calorimeter (DSC) for direct thermal characterization of protein samples. The DSC consisted of a pair of temperature sensors made by vanadium oxide (VOx) film with a temperature coefficient of resistivity of –0.025/K at 300 K, a microfluidic device with high thermal insulation (2.8 K/mW), and a Peltier heater for linear temperature scanning. The DSC exhibited high sensitivity (6.1 µV/µW), low noise (0.4 µW), high scanning rate (45 K/min), and low sample consumption volume (0.63 µL). The MEMS DSC was verified by measuring the temperature-induced denaturation of lysozyme at different pH, and then used to study the thermal stability of a monoclonal antibody (mAb), an antigen-binding fragment (Fab), and a dual variable domain immunoglobulin (DVD-Ig) at pH = 6. The results showed that lysozyme is a stable protein in the pH range of 4.0–8.0. The protein stability study revealed that the transition temperatures of the intact Fab fragment, mAb, and DVD proteins were comparable with conformational stability results obtained using conventional commercial DSC. These studies demonstrated that the MEMS DSC is an effective tool for directly understanding the thermal stability of antibodies in a high-throughput and low-cost manner compared to conventional calorimeters.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2020

Growth and Characterization of Arsenic-Doped CdTe 1-x Se x Single Crystals Grown by the Cd-Solvent Traveling Heater Method

The photovoltaic performance of CdTe solar cells is mainly limited by low doping and short minority carrier lifetime. Group-V element doping and Se-alloying have a significant impact on tuning these fundamental CdTe properties. In this paper, we report the growth of p-type As-doped, Cd-rich CdTe 1-x Se x single crystals using metallic Cd as the solvent in the traveling-heater method. The structural and electrical properties of CdTe1-xSex are examined for different Se concentrations. CdTe 1-x Se x single crystals (0 ≤ x ≤ 0.5) with zincblende structure indicate homogeneous composition. The 10 17 cm-3 As-doping activation efficiency can be maintained at close to 50% for x ≤ 0.2. Se alloying leads to bulk minority carrier lifetime exceeding 30 ns for samples doped near 1017 cm -3 . These results help us to overcome the current roadblocks in device performance.

14 SOLAR ENERGY↗

DOE OSTI2021

Smartphone-based Dual-channel Immunochromatographic Test Strip with Polymer Quantum Dot Labels for Simultaneous Detection of Cypermethrin and 3-phenoxybenzoic acid

Currently, gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-mass spectrometry (LC-MS) are the primary methods used to detect pesticides and their metabolites for biomonitoring of exposure. Although GC-MS and LC-MS can provide accurate and sensitive measurements, these techniques are not suitable for point-of-care or in-field biomonitoring applications. The objective of this work is to develop a smartphone-based dual-channel immunochromatographic test strip (ICTS) for on-site biomonitoring of exposure to cypermethrin by simultaneous detection of cypermethrin and its metabolite, 3-phenoxybenzoic acid (3-PBA). Polymer carbon dots (PCDs) with ultra-high fluorescent brightness were synthesized and used as signal amplifier in ICTS assay. Cypermethrin (a representative pyrethroid pesticide) and its major metabolite 3-PBA were simultaneously detected to provide more comprehensive analysis of cypermethrin exposure. After competitive immunoreactions between the target sample and the coating antigens preloaded on the test line, the tracer antibody (PCDs conjugated antibody) was quantitatively captured on the test lines. The captured PCDs were inversely proportional to the amount of the target compound in sample. The red fluorescence on the test line then was recorded by a smartphone-based device capable of conducting image analysis and recording. Under optimal conditions, the sensor showed excellent linear responses for detecting cypermethrin and 3-PBA ranging from 1 ng/mL to 100 ng/mL and from 0.1 ng/mL to 100 ng/mL, the limits of detection were calculated to be ~0.35 ng/mL for cypermethrin and ~0.04 ng/mL for 3-PBA, respectively. The results demonstrate that the ICTS device is promising for accurate point-of-care biomonitoring of pesticide exposure.

Zhao, Yuting↗

DOE OSTI2020

Depth Thermography: Noninvasive 3D Temperature Profiling Using Infrared Thermal Emission

Here, we introduce a technique based on infrared thermal emission, termed depth thermography, that can remotely measure the temperature distribution beneath the surface of certain objects. Depth thermography utilizes the thermal-emission spectrum in the semitransparent spectral region of the target object to extract its temperature as a function of depth, in contrast with conventional thermography, which uses the spectrally integrated thermally emitted power to measure the surface temperature. Coupled with two-dimensional imaging, for example using an infrared hyperspectral camera or scanning a single-pixel spectrometer, this technique can yield volumetric temperature distributions. Furthermore, we carried out a proof-of-concept experiment on an asymmetrically heated fused-silica window, extracting the temperature distribution throughout the sample. Depth thermography may enable noncontact volumetric temperature measurements of microscopic objects such as multilayer electronic devices or macroscopic volumes of liquids and gases, as well as simultaneous all-optical measurements of optical and thermal properties of materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2023

Spatially-resolved dynamic sampling of different phasic magnetic resonances of nanoparticle ensembles in a magnetotactic bacterium Magnetospirillum magnetotacticum

Abstract Nanoscaled magnetic particle ensembles are promising building blocks for realizing magnon based binary logic. Element-specific real-space monitoring of magnetic resonance modes with sampling rates in the GHz regime is imperative for the experimental verification of future complex magnonic devices. Here we present the observation of different phasic magnetic resonance modes using the element-specific technique of time-resolved scanning transmission x-ray microscopy within a chain of dipolarly coupled Fe 3 O 4 nanoparticles (40–50 nm particle size) inside a single cell of a magnetotactic bacterium Magnetospirillum magnetotacticum . The particles are probed with 25 nm resolution at the Fe L 3 x-ray absorption edge in response to a microwave excitation of 4.07 GHz. A plethora of resonance modes is observed within multiple particle segments oscillating in- and out-of-phase, well resembled by micromagnetic simulations.

time-resolved scanning transmission x-ray microsco↗

NASA NTRS1988

Temporal evolution of collisionless sheaths

Experimental measurements have been performed to determine the temporal evolution of Langmuir sheaths near an electrode to which a negative step bias is applied in a collisionless argon plasma. The plasma was produced by a hot-filament discharge in a multidipole device. Plasma potential data were obtained using emissive probes with two different techniques: time-resolved sampling and time-averaged techniques. The sheath is found to initially form close to the electrode, to extend to a maximum separation, and to contract to a steady-state value. The time scale required to reach a steady state is close to the time scale of the presheath relaxation. Characteristics of sheaths in RF plasmas are also measured using a parallel-plate plasma capacitor. It is observed that the plasma potential profile has significant variation with frequency, even for frequencies as low as 1 kHz which are far below the ion plasma frequency (about 1 MHz).

Cho, M. H.↗

NASA NTRS1993

Multiresponse Imaging For Improved Resolution

Images restored with resolution finer than sampling lattice. Multiresponse imaging overcomes sampling-passband constraint and critically constrained only by optical response and sensitivity of image-gathering device. Process consists of multiresponse image gathering and Wiener-matrix restoration. Image-gathering process acquires sequence of images, each with different optical response so within-pass-band and aliased signal components weighted differently. Wiener-matrix filter, in turn, unscrambles within-passband and aliased frequency components of undersampled signal and restores them up to cutoff frequency of optical response.

Fales, Carl L., Jr.↗

NASA NTRS1994

Issues on Reproducibility/Reliability of Magnetic NDE Methods

One of the critical elements related to the practicality of any NDE technique is its reproducibility under nominally the same inspection conditions. The results of certain test methodologies, however, are not always repeatable and understanding the origin of the irreproducibility is often as critical as obtaining reproducible results. One example is the characterization of residual stress in structural ferromagnets using the magnetoacoustic (MAC) method. Although it has not been widely publicized, the test results of this method are known to be time-dependent. Two distinct types of time dependencies have been observed during testing. The first type has a clearly definable relaxation time, while no such trend has been observed for the second. The purpose of the present study is to systematically investigate the time dependence of the second type, to find out the range and, if possible, the origin of the variation in the test results. For this, MAC curves were obtained under various stress levels and the tests were repeated over time. Particular attention was given to whether noise in the measuring device or a change in the laboratory environment could have been a contributing factor. The steel samples used for the study were cut from C- and U-class railroad wheels. The MAC behavior of these samples was reported previously. Each steel sample was first machined to be a cylindrical rod of 3.175 cm (1.25 in) in diameter and 26.67 cm (10.5 in) in length. The center portion of the samples were further machined to form a pair of flat and parallel surfaces for the launch and reflection of the ultrasonic pulses. Data acquisition involved two major elements; magnetic and acoustic measurements. Throughout the experiment the net magnetic induction, B, was measured by integrating the induction pickup coil output using an integrating fluxmeter. The acoustic measurements employed the phase-locked technique which will be described in the following.

Namkung, M.↗

NASA NTRS2009

Electrical Arc Ignition Testing for Constellation Program

NASA Johnson Space Center (JSC) Materials and Processes Branch requested that NASA JSC White Sands Test Facility (WSTF) perform testing for the Constellation Program to evaluate the hazard of electrical arc ignition of materials that could be in close proximity to batteries. Specifically, WSTF was requested to perform wire-break electrical arc tests to determine the current threshold for ignition of generic cotton woven fabric samples with a fixed voltage of 3.7 V, a common voltage for hand-held electrical devices. The wire-break test was developed during a previous test program to evaluate the hazard of electrical arc ignition inside the Extravehicular Mobility Unit [1].

Sparks, Kyle↗

NASA NTRS2014

Rapid Electrochemical Detection and Identification of Microbiological and Chemical Contaminants for Manned Spaceflight Project

Microbial control in the spacecraft environment is a daunting task, especially in the presence of human crew members. Currently, assessing the potential crew health risk associated with a microbial contamination event requires return of representative environmental samples that are analyzed in a ground-based laboratory. It is therefore not currently possible to quickly identify microbes during spaceflight. This project addresses the unmet need for spaceflight-compatible microbial identification technology. The electrochemical detection and identification platform is expected to provide a sensitive, specific, and rapid sample-to-answer capability for in-flight microbial monitoring that can distinguish between related microorganisms (pathogens and non-pathogens) as well as chemical contaminants. This will dramatically enhance our ability to monitor the spacecraft environment and the health risk to the crew. Further, the project is expected to eliminate the need for sample return while significantly reducing crew time required for detection of multiple targets. Initial work will focus on the optimization of bacterial detection and identification. The platform is designed to release nucleic acids (DNA and RNA) from microorganisms without the use of harmful chemicals. Bacterial DNA or RNA is captured by bacteria-specific probe molecules that are bound to a microelectrode, and that capture event can generate a small change in the electrical current (Lam, et al. 2012. Anal. Chem. 84(1): 21-5.). This current is measured, and a determination is made whether a given microbe is present in the sample analyzed. Chemical detection can be accomplished by directly applying a sample to the microelectrode and measuring the resulting current change. This rapid microbial and chemical detection device is designed to be a low-cost, low-power platform anticipated to be operated independently of an external power source, characteristics optimal for manned spaceflight and areas where power and computing resources are scarce.

Pierson, Duane↗

DOE OSTI2020

Device and system for selective ionization and analyte detection and method of using the same

Disclosed herein are embodiments of a system for selectively ionizing samples that may comprise a plurality of different analytes that are not normally detectable using the same ionization technique. The disclosed system comprises a unique split flow tube that can be coupled with a plurality of ionization sources to facilitate using different ionization techniques for the same sample. Also disclosed herein are embodiments of a method for determining the presence of analytes in a sample, wherein the number and type of detectable analytes that can be identified is increased and sensitivity and selectivity are not sacrificed.

45 MILITARY TECHNOLOGY, WEAPONRY, AND NATIONAL DEF↗

DOE OSTI2021

Device and system for selective ionization and analyte detection and method of using the same

Denis, Elizabeth↗

NASA NTRS1980

The hammer QSD-quick stop device for high speed machining and rubbing

A quick stop device (QSD) was designed for use in orthogonal machining and rubbing experiments. QSD's are used to obtain chip root samples that are representative of the deformation taking place during dynamic (actual) cutting conditions. These 'frozen' specimens are helpful in examining the plastic deformation that occurs in the regions of compression and shear which form the chip; the secondary shear at the tool-chip interface; and the nose ploughing/flank rubbing action which operates on the newly machined surface. The Hammer QSD employs a shear pin mechanism, broken by a flying hammer, which is traveling at the same velocity as the workpiece. The device has been successfully tested up to 6000 sfpm (30.48 m/sec).

Black, J. T.↗

DOE OSTI2023

High-throughput feedback-enabled optogenetic stimulation and spectroscopy in microwell plates

Abstract The ability to perform sophisticated, high-throughput optogenetic experiments has been greatly enhanced by recent open-source illumination devices that allow independent programming of light patterns in single wells of microwell plates. However, there is currently a lack of instrumentation to monitor such experiments in real time, necessitating repeated transfers of the samples to stand-alone analytical instruments, thus limiting the types of experiments that could be performed. Here we address this gap with the development of the optoPlateReader (oPR), an open-source, solid-state, compact device that allows automated optogenetic stimulation and spectroscopy in each well of a 96-well plate. The oPR integrates an optoPlate illumination module with a module called the optoReader, an array of 96 photodiodes and LEDs that allows 96 parallel light measurements. The oPR was optimized for stimulation with blue light and for measurements of optical density and fluorescence. After calibration of all device components, we used the oPR to measure growth and to induce and measure fluorescent protein expression in E. coli . We further demonstrated how the optical read/write capabilities of the oPR permit computer-in-the-loop feedback control, where the current state of the sample can be used to adjust the optical stimulation parameters of the sample according to pre-defined feedback algorithms. The oPR will thus help realize an untapped potential for optogenetic experiments by enabling automated reading, writing, and feedback in microwell plates through open-source hardware that is accessible, customizable, and inexpensive.

59 BASIC BIOLOGICAL SCIENCES↗

NASA NTRS2016

Characterization of Carbon Dioxide Washout Measurement Techniques in the Mark-III Space Suit

Providing adequate carbon dioxide (CO2) washout is essential to the reduction of risk in performing suited operations. Long term CO2 exposure can lead to symptoms such as headache, lethargy, dizziness, and in severe cases can lead to unconsciousness and death. Thus maintaining adequate CO2 washout in both ground testing and during in flight EVAs is a requirement of current and future suit designs. It is necessary to understand the inspired CO2 of suit wearers such that future requirements for space suits appropriately address the risk of inadequate washout. Testing conducted by the EVA Physiology Laboratory at the NASA Johnson Space Center aimed to characterize a method for noninvasively measuring inspired oronasal CO2 under pressurized suited conditions in order to better inform requirements definition and verification techniques for future CO2 washout limits in space suits. Prior work conducted by the EPL examined several different wearable, respirator style, masks that could be used to sample air from the vicinity surround the nose and mouth of a suited test subject. Previously published studies utilized these masks, some being commercial products and some novel designs, to monitor CO2 under various exercise and flow conditions with mixed results for repeatability and/or consistency between subjects. Based on a meta-analysis of those studies it was decided to test a nasal cannula as it is a commercially available device that is placed directly in the flow path of the user as they breathe. A nasal cannula was used to sample air inhaled by the test subjects during both rest and exercise conditions. Eight subjects were tasked with walking on a treadmill or operating an arm ergometer to reach target metabolic rates of 1000, 2000, and 3000 BTU/hr. Suit pressure was maintained at 4.3 psid for all tests, with supply flow rates of 6, 4, and 2 actual cubic feet per minute depending on the test condition. Each test configuration was conducted twice with subjects breathing either through their nose only, or however they felt comfortable. By restricting breathing through a single orifice, we are able to more accurately define exactly what flow stream the sampled CO2 is taken from. Oronasal CO2 was monitored using real time infrared gas analyzers fed via sample tubes connected to the nasal cannula within the suit. Two additional sampling tubes were placed at the head and chin of the test subject, in an effort to capture CO2 concentrations across the entire flow stream of the Mark-III vent system (flow path is head to neck). Metabolic rate was calculated via the exhaust CO2 concentration and used to adjust subject workload on either the treadmill or arm ergometer until the target was reached. Forward work will aim to characterize the historically accepted minimum ppCO2 in suit during EVA by repeating this study in the Extravehicular Mobility Unit (EMU) space suit. This will help to define washout requirements for future suits, be they NASA (e.g. Z-2) or Commercial Crew designed. Additionally it is important to determine the functional consequences of CO2 exposure during EVA. Severe CO2 symptoms are a result of very high concentration, acute exposures. While long term, low concentration exposures have been shown to result in slight cognitive decline, symptoms resolve upon quickly returning to nominal concentrations and it remains unknown the impact that minor deficits in cognitive performance can have on EVA performance.

Norcross, J.↗

NASA NTRS2002

Specification and Design of the SBRC-190: A Cryogenic Multiplexer for Far Infrared Photoconductor Detectors

Arrays of far-infrared photoconductor detectors operate at a few degrees Kelvin and require electronic amplifiers in close proximity. For the electronics, a cryogenic multiplexer is ideal to avoid the large number of wires associated with individual amplifiers for each pixel, and to avoid adverse effects of thermal and radiative heat loads from the circuitry. For low background applications, the 32 channel CRC 696 CMOS device was previously developed for SIRTF, the cryogenic Space Infrared Telescope Facility. For higher background applications, we have developed a similar circuit, featuring several modifications: (a) an AC coupled, capacitive feedback transimpedence unit cell, to minimize input offset effects, thereby enabling low detector biases, (b) selectable feedback capacitors to enable operation over a wide range of backgrounds, and (c) clamp and sample & hold output circuits to improve sampling efficiency, which is a concern at the high readout rates required. We describe the requirements for and design of the new device.

Erickson, E. F.↗

DOE OSTI2022

Development of an operando characterization stage for multi-modal synchrotron x-ray experiments

It is widely accepted that micro- and nanoscale inhomogeneities govern the performance of many thin-film solar cell absorbers. These inhomogeneities yield material properties (e.g., composition, structure, and charge collection) that are challenging to correlate across length scales and measurement modalities. The challenge is compounded if a correlation is sought during device operation or in conditions that mimic aging under particular stressors (e.g., heat and electrical bias). Correlative approaches, particularly those based on synchrotron x-ray sources, are powerful since they can access several material properties in different modes (e.g., fluorescence, diffraction, and absorption) with minimal sample preparation. Small-scale laboratory x-ray instruments have begun to offer multi-modality but are typically limited by low x-ray photon flux, low spatial resolution, or specific sample sizes. To overcome these limitations, a characterization stage was developed to enable multi-scale, multi-modal operando measurements of industrially relevant photovoltaic devices. The stage offers compatibility across synchrotron x-ray facilities, enabling correlation between nanoscale x-ray fluorescence microscopy, microscale x-ray diffraction microscopy, and x-ray beam induced current microscopy, among others. Furthermore, the stage can accommodate device sizes up to 25 × 25 mm 2 , offering access to multiple regions of interest and increasing the statistical significance of correlated properties. The stage materials can sustain humid and non-oxidizing atmospheres, and temperature ranges encountered by photovoltaic devices in operational environments (e.g., from 25 to 100 °C). As a case study, we discuss the functionality of the stage by studying Se-alloyed CdTe photovoltaic devices aged in the stage between 25 and 100 °C.

14 SOLAR ENERGY↗

NASA NTRS2007

Liquid Metering Centrifuge Sticks (LMCS): A Centrifugal Approach to Metering Known Sample Volumes for Colorimetric Solid Phase Extraction (C-SPE)

Phase separation is one of the most significant obstacles encountered during the development of analytical methods for water quality monitoring in spacecraft environments. Removing air bubbles from water samples prior to analysis is a routine task on earth; however, in the absence of gravity, this routine task becomes extremely difficult. This paper details the development and initial ground testing of liquid metering centrifuge sticks (LMCS), devices designed to collect and meter a known volume of bubble-free water in microgravity. The LMCS uses centrifugal force to eliminate entrapped air and reproducibly meter liquid sample volumes for analysis with Colorimetric Solid Phase Extraction (C-SPE). C-SPE is a sorption-spectrophotometric platform that is being developed as a potential spacecraft water quality monitoring system. C-SPE utilizes solid phase extraction membranes impregnated with analyte-specific colorimetric reagents to concentrate and complex target analytes in spacecraft water samples. The mass of analyte extracted from the water sample is determined using diffuse reflectance (DR) data collected from the membrane surface and an analyte-specific calibration curve. The analyte concentration can then be calculated from the mass of extracted analyte and the volume of the sample analyzed. Previous flight experiments conducted in microgravity conditions aboard the NASA KC-135 aircraft demonstrated that the inability to collect and meter a known volume of water using a syringe was a limiting factor in the accuracy of C-SPE measurements. Herein, results obtained from ground based C-SPE experiments using ionic silver as a test analyte and either the LMCS or syringes for sample metering are compared to evaluate the performance of the LMCS. These results indicate very good agreement between the two sample metering methods and clearly illustrate the potential of utilizing centrifugal forces to achieve phase separation and metering of water samples in microgravity.

Gazda, Daniel B.↗